Operation and calibration procedures of gas chromatograph
Operation and calibration procedures of gas chromatograph
To provide the operation and calibration procedures of the gas chromatograph.
Is applicable to the operation and calibration procedures of gas chromatographs.
The quality Control Analyst shall be responsible to follow the procedure mentioned in this SOP.
QC Head and QA Head shall be accountable for compliance with this SOP.
ATTACHMENTS
Calibration format for gas chromatograph – Attachment I
PROCEDURE
Measurement procedure
- Ensure that the instrument is clean and free from dust.
- Connect the chromatographic column.
- Turn on the air, hydrogen, and nitrogen/helium supply system.
- Switch on the instrument using the POWER key on the side panel. Turn on the auto-injector with ON/OFF.
- Switch on the computer and open GC Solution software. Select the instrument, enter the password and click OK. GC Real-Time Analysis program is started.
- Set the conditions – temperature, rate, split ratio etc. – or select already existed method. Set the parameters of sample preparation (Tools tab).
- Press the System On key to start the instrument.
- Click Download to send the settings to the instrument.
- On Batch Processing window set the sequence of injections.
- Wait till READY appears on the display.
- Place the vials with samples into the corresponding cells.
- Start the analysis by clicking Start on the Batch Processing window.
- After completion of the analysis open the Post run window in GC Solution software to process the results.
- Close the software 20-30 min. after the completion of the analysis. Switch off the instrument using the POWER key on the side panel. Turn off the auto-injector with ON/OFF. Turn off the air, hydrogen and nitrogen/helium supply system.
Calibration procedure
- Carry out the analysis at the following conditions:
- Column – AB-624 (0.53 мм/mm х 30м/m х 3 мкм/µm).
- Initial column temperature – 100 °C.
- Initial time- 0 min.
- Rate of heating – 10°С /min.
- Final column temperature- 150°C.
- Final time– 5 min.
- Injector temperature- 250°C.
- Detector temperature – 270°C.
- Split ration – 1:10.
- Purge flow – 3 ml/min.
- Injection volume – 1 µl.
- Preparation of solutions.
- Blank solution – methanol.
- Standard solution – Dilute 500 mg of toluene and 500 mg of dimethylformamide to 50 ml with methanol.
- The sequence of injections:
- blank solution- х1;
- standard solution – x6.
- Acceptance criteria.
- Peak retention times: toluene – 5.5-6.5 min., dimethylformamide – 6.5-7.5 min.
- RSD calculated due to the retention times is not more than 2%.
- RSD calculated due to relative retention times of toluene/dimethylformamide is not more than 2%.
- Frequency of calibration.
- Every 6 months and after detector or injector repair.
- Maintenance and safety instructions.
- Keep the instrument in the place free from dust, corrosive acid vapors and excessive humidity and temperatures. This place must be protected from vibration and direct sun lights.
- Be careful when handling those instrument parts which got hot.
- Take thorough measures to prevent buildup of static electricity.
- Do not keep highly inflammable materials near the instrument.
- Follow the safety engineering rules when working with hydrogen and nitrogen.
- Wipe the instrument with the dry tissue. If necessary, use the detergent.
REFERENCES
- In-house
ABBREVIATIONS
- QC: Quality Control Department
- QA: Quality Assurance Department
- RSD: /Relative Standard Deviation
DISTRIBUTION LIST
- Quality Control Department
- Quality Assurance Department
HISTORY OF REVISION
Attachment I
Calibration format for gas chromatograph
Date of calibration: Due date of calibration:
Model: I.D.No:
Frequency: once in 6 months (+7 days)
Sr. No | Limits of RT of toluene (min.) | RT of toluene ВУ | RSD(RT of toluene) NMT 2.0% | Limits RT of DMF (min.) | RT of DMF ВУ | RSD (RT of DMF) NMT 2.0% | RRT Toluene/DMF ОВУ | RSD (RRT toluene/DMF NMT 2.0% ОСО (ОВУ |
1 | 5,5 – 6,5 | 6.5 – 7,5 | ||||||
2 | 5,5 – 6,5 | 6.5 – 7,5 | ||||||
3 | 5,5 – 6,5 | 6.5 – 7,5 | ||||||
4 | 5,5 – 6,5 | 6.5 – 7,5 | ||||||
5 | 5,5 – 6,5 | 6.5 – 7,5 | ||||||
6 | 5,5 – 6,5 | 6.5 – 7,5 |